Hydrochloric Acid → N-(1.4-Dihydro-6.7-dichloro-2.3-dioxoquinoxaline-5-yl)-N-(3-pyridylmethyl)methanesulphonamide hydrochloride

HRID 1458556노트

반응식

HRID 1458556 반응식
[Cl:1][C:2]1[C:3]([N:17]([CH2:22][C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[S:18]([CH3:21])(=[O:20])=[O:19])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[N:8]=[C:7]([O:13]C)[C:6]([O:15]C)=[N:5]2.Cl>O1CCOCC1>[ClH:1].[Cl:1][C:2]1[C:3]([N:17]([CH2:22][C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[S:18]([CH3:21])(=[O:20])=[O:19])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:15])[NH:5]2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22097013N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(3-pyridylmethyl)methanesulphonamide

생성물 1

HCID 22097005N-(1.4-Dihydro-6.7-dichloro-2.3-dioxoquinoxaline-5-yl)-N-(3-pyridylmethyl)methanesulphonamide hydrochloride수율 181.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(3-pyridylmethyl)-methanesulphonamide (130 mg, 0.293 mmol), 2M hydrochloric acid (2 ml) and dioxane (4 ml) was heated at reflux for 2.5 hours, cooled, and concentrated under reduced pressure. The residue was suspended in water (1 ml), filtered off, and washed with water and ether to give the title compound (120 mg, 98%) as a white solid, m.p. 234°-235° C. (dec.).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hours
  3. temperaturecooled
  4. concentrationconcentrated under reduced pressure
  5. filtrationfiltered off
  6. washwashed with water and ether

출처 및 근거

ORD 기록
ord-115a64dcec294303b602f2f6f711fc17
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05852016

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